#------------------------------------------------------------------------------
#$Date: 2022-01-18 00:49:58 +0200 (Tue, 18 Jan 2022) $
#$Revision: 272085 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/95/7129584.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7129584
loop_
_publ_author_name
'Fontana, Nicolò'
'Espinosa-Jalapa, Noel Angel'
'Seidl, Michael'
'Bauer, Jonathan O.'
_publ_section_title
;
 Hidden Silylium-Type Reactivity of a Siloxane-Based
 Phosphonium--Hydroborate Ion Pair
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC07016A
_journal_year                    2022
_chemical_formula_moiety         'C31 H44 O P S Si2, B C24 F20'
_chemical_formula_sum            'C55 H44 B F20 O P S Si2'
_chemical_formula_weight         1230.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-14
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_audit_update_record
;
2021-09-02 deposited with the CCDC.	2022-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                101.2990(10)
_cell_angle_beta                 90.3210(10)
_cell_angle_gamma                93.8460(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9141(2)
_cell_length_b                   14.3805(2)
_cell_length_c                   19.1892(3)
_cell_measurement_reflns_used    23003
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      66.4750
_cell_measurement_theta_min      4.2760
_cell_volume                     2676.24(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00 -42.00   1.00    5.00    --  -42.98  78.00  22.00   26
  2  ω     -5.00  20.00   1.00    5.00    --  -42.98  78.00  22.00   25
  3  ω    -30.00  36.00   1.00    5.00    --   42.98 -78.00-102.00   66
  4  ω     49.00  75.00   1.00    5.00    --   42.98 -78.00-102.00   26
  5  ω     41.00  66.00   1.00   30.00    --   86.50 -78.00-102.00   25
  6  ω   -163.00-114.00   1.00   30.00    --  -90.00 -78.00-102.00   49
  7  ω    -93.00 -29.00   1.00    5.00    --  -42.98 125.00 150.00   64
  8  ω     42.00 113.00   1.00    5.00    --   42.98  57.00  30.00   71
  9  ω     29.00 107.00   1.00    5.00    --   42.98  57.00 -30.00   78
 10  ω     96.00 121.00   1.00   30.00    --   86.50  78.00  22.00   25
 11  ω   -112.00 -55.00   1.00   30.00    --  -90.00 125.00 150.00   57
 12  ω   -105.00 -35.00   1.00   30.00    --  -90.00 125.00  30.00   70
 13  ω   -164.00-103.00   1.00   30.00    --  -90.00 -77.00   0.00   61
 14  ω   -106.00 -67.00   1.00   30.00    --  -90.00 110.00  15.87   39
 15  ω    -68.00 -42.00   1.00   30.00    --  -90.00  15.00  60.00   26
 16  ω    -60.00 -15.00   1.00   30.00    --  -90.00 110.00  15.87   45
 17  ω   -173.00-147.00   1.00   30.00    --  -90.00 -94.00-120.00   26
 18  ω    -99.00 -28.00   1.00   30.00    --  -90.00 125.00-180.00   71
 19  ω   -112.00 -51.00   1.00   30.00    --  -90.00 125.00  60.00   61
 20  ω    -67.00 -42.00   1.00   30.00    --  -90.00  45.00  30.00   25
 21  ω    -63.00 -31.00   1.00   30.00    --  -90.00  99.00-174.74   32
 22  ω   -116.00 -62.00   1.00   30.00    --  -90.00  61.00 -30.00   54
 23  ω   -163.00-132.00   1.00   30.00    --  -90.00 -77.00  60.00   31
 24  ω   -107.00 -30.00   1.00   30.00    --  -90.00 125.00 -90.00   77
 25  ω   -125.00 -97.00   1.00   30.00    --  -90.00-125.00 -30.00   28
 26  ω   -145.00-107.00   1.00   30.00    --  -90.00 -77.00 150.00   38
 27  ω   -131.00-105.00   1.00   30.00    --  -90.00 151.00-103.36   26
 28  ω    -90.00 -32.00   1.00   30.00    --  -90.00  53.00 -98.49   58
 29  ω   -110.00 -85.00   1.00   30.00    --  -90.00 -45.00  90.00   25
 30  ω   -138.00-113.00   1.00   30.00    --  -90.00 -94.00-120.00   25
 31  ω    -94.00 -42.00   1.00   30.00    --  -90.00 125.00  90.00   52
 32  ω   -105.00 -80.00   1.00   30.00    --  -90.00  77.00  60.00   25
 33  ω    -72.00 -46.00   1.00   30.00    --  -90.00  77.00  60.00   26
 34  ω   -122.00 -92.00   1.00   30.00    --  -90.00  83.00  10.63   30
 35  ω    -42.00 -17.00   1.00   30.00    --  -90.00  83.00  10.63   25
 36  ω   -144.00-104.00   1.00   30.00    --  -90.00 -94.00  41.29   40
 37  ω   -142.00-116.00   1.00   30.00    --  -90.00-125.00  30.00   26
 38  ω    -72.00 -47.00   1.00   30.00    --  -90.00  86.00 -35.32   25
 39  ω   -121.00 -96.00   1.00   30.00    --  -90.00  86.00 -35.32   25
 40  ω   -164.00-138.00   1.00   30.00    --  -90.00-125.00 -60.00   26
 41  ω   -125.00 -98.00   1.00   30.00    --  -90.00-125.00 -60.00   27
 42  ω   -107.00 -31.00   1.00   30.00    --  -90.00 125.00 120.00   76
 43  ω    -77.00 -31.00   1.00   30.00    --  -90.00  45.00 -30.00   46
 44  ω   -107.00 -66.00   1.00   30.00    --  -90.00 -61.00   0.00   41
 45  ω    -61.00 -26.00   1.00   30.00    --  -90.00  30.00 -30.00   35
 46  ω   -157.00-131.00   1.00   30.00    --  -90.00 -77.00 120.00   26
 47  ω   -162.00-110.00   1.00   30.00    --  -90.00-125.00-180.00   52
 48  ω   -162.00-128.00   1.00   30.00    --  -90.00-125.00   0.00   34
 49  ω    -69.00 -37.00   1.00   30.00    --  -90.00 125.00-150.00   32
 50  ω   -143.00-117.00   1.00   30.00    --  -90.00 -45.00-150.00   26
 51  ω    -93.00 -66.00   1.00   30.00    --  -90.00 -45.00  60.00   27
 52  ω   -160.00-126.00   1.00   30.00    --  -90.00 -45.00  90.00   34
 53  ω   -115.00 -73.00   1.00   30.00    --  -90.00  15.00  60.00   42
 54  ω   -107.00 -82.00   1.00   30.00    --  -90.00  61.00-120.00   25
 55  ω   -108.00 -82.00   1.00   30.00    --  -90.00 103.00 -80.98   26
 56  ω    -76.00 -51.00   1.00   30.00    --  -90.00  96.00  79.02   25
 57  ω    -98.00 -73.00   1.00   30.00    --  -90.00  89.00 149.38   25
 58  ω    -38.00 -13.00   1.00   30.00    --  -90.00  89.00 149.38   25
 59  ω    -45.00 -20.00   1.00   30.00    --  -90.00  30.00 -60.00   25
 60  ω    -87.00 -62.00   1.00   30.00    --  -90.00  27.00 178.81   25
 61  ω    -97.00 -71.00   1.00   30.00    --  -90.00  78.00  22.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, TitanS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1061468000
_diffrn_orient_matrix_UB_12      -0.0420058000
_diffrn_orient_matrix_UB_13      -0.0532908000
_diffrn_orient_matrix_UB_21      0.1120107000
_diffrn_orient_matrix_UB_22      0.0650697000
_diffrn_orient_matrix_UB_23      0.0444414000
_diffrn_orient_matrix_UB_31      0.0212332000
_diffrn_orient_matrix_UB_32      -0.0774213000
_diffrn_orient_matrix_UB_33      0.0434759000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41863
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.647
_diffrn_reflns_theta_max         66.647
_diffrn_reflns_theta_min         4.278
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.247
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             1252
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/pentane'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         9402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0804P)²+1.5416P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8248
_reflns_number_total             9402
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc07016a2.cif
_cod_data_source_block           nf_693_1_ap_abs_ana
_cod_database_code               7129584
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C55H44BF20OPSSi2
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.650
_shelx_estimated_absorpt_t_min   0.507
_reflns_odcompleteness_completeness 98.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C21(H21), C11(H11), C15(H15), C13(H13), C12(H12), C27(H27),
 C17(H17), C23(H23), C20(H20), C19(H19), C26(H26), C18(H18), C25(H25), C24(H24)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C9(H9A,H9B,H9C), C5(H5A,H5B,H5C),
 C8(H8A,H8B,H8C), C31(H31A,H31B,H31C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,
 H7B,H7C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.145
_oxdiff_exptl_absorpt_empirical_full_min 0.097
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 1.02242(6) 0.74252(4) 0.79450(3) 0.02557(15) Uani 1 1 d . . . . .
P1 P 0.83572(6) 0.67149(4) 0.80038(3) 0.02132(15) Uani 1 1 d . . . . .
Si1 Si 0.83322(6) 0.59507(4) 0.62782(3) 0.01999(15) Uani 1 1 d . . . . .
Si2 Si 1.05568(6) 0.75093(4) 0.68290(3) 0.02034(15) Uani 1 1 d . . . . .
F10 F 0.28482(14) 0.29394(10) 0.94229(7) 0.0258(3) Uani 1 1 d . . . . .
F7 F 0.44280(15) 0.50495(10) 0.74795(7) 0.0295(3) Uani 1 1 d . . . . .
F6 F 0.50495(14) 0.32634(10) 0.72844(7) 0.0251(3) Uani 1 1 d . . . . .
F11 F 0.56516(14) 0.04342(10) 0.89263(7) 0.0289(3) Uani 1 1 d . . . . .
F16 F 0.54593(14) 0.23988(11) 0.96183(7) 0.0299(3) Uani 1 1 d . . . . .
F20 F 0.69950(14) 0.19735(10) 0.72481(7) 0.0287(3) Uani 1 1 d . . . . .
F15 F 0.15453(14) 0.16331(10) 0.83324(8) 0.0298(3) Uani 1 1 d . . . . .
F1 F 0.58363(15) 0.02427(10) 0.74480(7) 0.0306(3) Uani 1 1 d . . . . .
F5 F 0.24067(15) 0.22555(10) 0.70767(7) 0.0314(3) Uani 1 1 d . . . . .
F19 F 0.94491(15) 0.26170(11) 0.77320(9) 0.0376(4) Uani 1 1 d . . . . .
F9 F 0.22715(16) 0.47394(11) 0.96120(8) 0.0359(4) Uani 1 1 d . . . . .
F8 F 0.30197(16) 0.58298(10) 0.86475(8) 0.0354(4) Uani 1 1 d . . . . .
F14 F 0.01779(16) 0.03974(12) 0.89786(9) 0.0396(4) Uani 1 1 d . . . . .
F4 F 0.19756(17) 0.12509(12) 0.57826(8) 0.0401(4) Uani 1 1 d . . . . .
F12 F 0.42670(18) -0.08369(11) 0.95063(8) 0.0399(4) Uani 1 1 d . . . . .
F2 F 0.54477(19) -0.07123(11) 0.61201(8) 0.0430(4) Uani 1 1 d . . . . .
O1 O 0.97673(17) 0.65956(11) 0.63193(8) 0.0236(4) Uani 1 1 d . . . . .
F3 F 0.3494(2) -0.02405(13) 0.52652(8) 0.0476(4) Uani 1 1 d . . . . .
F18 F 0.99930(15) 0.31170(13) 0.91600(10) 0.0481(5) Uani 1 1 d . . . . .
F13 F 0.1518(2) -0.08714(12) 0.95664(9) 0.0459(4) Uani 1 1 d . . . . .
F17 F 0.79591(17) 0.29528(13) 1.00857(9) 0.0450(4) Uani 1 1 d . . . . .
C38 C 0.3933(2) 0.29720(16) 0.83217(11) 0.0198(5) Uani 1 1 d . . . . .
C16 C 0.8683(2) 0.46761(17) 0.60858(11) 0.0230(5) Uani 1 1 d . . . . .
C44 C 0.3674(2) 0.11392(16) 0.86143(11) 0.0212(5) Uani 1 1 d . . . . .
C49 C 0.2274(3) 0.10542(17) 0.86429(12) 0.0248(5) Uani 1 1 d . . . . .
C51 C 0.6427(2) 0.24043(17) 0.91236(13) 0.0245(5) Uani 1 1 d . . . . .
C43 C 0.3245(2) 0.34121(17) 0.89063(12) 0.0214(5) Uani 1 1 d . . . . .
C32 C 0.4197(2) 0.13308(16) 0.73354(12) 0.0215(5) Uani 1 1 d . . . . .
C39 C 0.4315(2) 0.35781(17) 0.78628(12) 0.0205(5) Uani 1 1 d . . . . .
C50 C 0.6080(2) 0.21231(16) 0.84064(12) 0.0211(5) Uani 1 1 d . . . . .
C10 C 0.7198(2) 0.62246(17) 0.55758(12) 0.0227(5) Uani 1 1 d . . . . .
C45 C 0.4291(2) 0.04681(17) 0.89232(12) 0.0230(5) Uani 1 1 d . . . . .
C48 C 0.1538(3) 0.04084(19) 0.89578(13) 0.0283(5) Uani 1 1 d . . . . .
C14 C 0.6133(3) 0.73942(19) 0.50439(13) 0.0278(5) Uani 1 1 d . . . . .
H14 H 0.589472 0.802893 0.507016 0.033 Uiso 1 1 calc R U . . .
C42 C 0.2935(2) 0.43611(18) 0.90299(13) 0.0255(5) Uani 1 1 d . . . . .
C33 C 0.4895(3) 0.05474(17) 0.70437(12) 0.0241(5) Uani 1 1 d . . . . .
C40 C 0.4009(2) 0.45180(17) 0.79594(12) 0.0234(5) Uani 1 1 d . . . . .
C21 C 0.7672(3) 0.39744(18) 0.61548(13) 0.0264(5) Uani 1 1 d . . . . .
H21 H 0.679630 0.415308 0.629957 0.032 Uiso 1 1 calc R U . . .
C1 C 0.7478(2) 0.63428(18) 0.71600(12) 0.0235(5) Uani 1 1 d . . . . .
H1A H 0.693249 0.687497 0.710050 0.028 Uiso 1 1 calc R U . . .
H1B H 0.682620 0.581059 0.721486 0.028 Uiso 1 1 calc R U . . .
C55 C 0.7159(2) 0.22008(17) 0.79616(13) 0.0246(5) Uani 1 1 d . . . . .
C54 C 0.8469(2) 0.25293(18) 0.81998(14) 0.0289(5) Uani 1 1 d . . . . .
C11 C 0.6813(3) 0.55385(18) 0.49735(13) 0.0260(5) Uani 1 1 d . . . . .
H11 H 0.703012 0.489951 0.494824 0.031 Uiso 1 1 calc R U . . .
C22 C 0.9918(2) 0.86389(17) 0.66786(13) 0.0240(5) Uani 1 1 d . . . . .
C15 C 0.6818(2) 0.71536(18) 0.56092(12) 0.0253(5) Uani 1 1 d . . . . .
H15 H 0.703184 0.762409 0.602335 0.030 Uiso 1 1 calc R U . . .
C47 C 0.2208(3) -0.02299(18) 0.92620(13) 0.0310(6) Uani 1 1 d . . . . .
C46 C 0.3587(3) -0.02032(17) 0.92287(12) 0.0293(6) Uani 1 1 d . . . . .
C37 C 0.3200(2) 0.15242(18) 0.68730(12) 0.0252(5) Uani 1 1 d . . . . .
C28 C 1.2425(2) 0.74757(18) 0.67297(13) 0.0271(5) Uani 1 1 d . . . . .
C13 C 0.5796(3) 0.6711(2) 0.44417(13) 0.0298(6) Uani 1 1 d . . . . .
H13 H 0.534676 0.688113 0.405111 0.036 Uiso 1 1 calc R U . . .
C12 C 0.6114(3) 0.57795(19) 0.44087(13) 0.0299(6) Uani 1 1 d . . . . .
H12 H 0.585592 0.530627 0.400250 0.036 Uiso 1 1 calc R U . . .
C27 C 0.9544(3) 0.87437(19) 0.59998(13) 0.0301(6) Uani 1 1 d . . . . .
H27 H 0.958799 0.822415 0.561120 0.036 Uiso 1 1 calc R U . . .
C52 C 0.7711(3) 0.27106(18) 0.93865(14) 0.0306(6) Uani 1 1 d . . . . .
C53 C 0.8745(3) 0.27791(19) 0.89159(15) 0.0330(6) Uani 1 1 d . . . . .
C17 C 0.9959(3) 0.43950(19) 0.58733(14) 0.0299(5) Uani 1 1 d . . . . .
H17 H 1.065595 0.486076 0.582010 0.036 Uiso 1 1 calc R U . . .
C34 C 0.4704(3) 0.00324(18) 0.63647(14) 0.0305(6) Uani 1 1 d . . . . .
C41 C 0.3310(3) 0.49122(17) 0.85442(13) 0.0260(5) Uani 1 1 d . . . . .
C35 C 0.3721(3) 0.02658(19) 0.59284(13) 0.0332(6) Uani 1 1 d . . . . .
C23 C 0.9865(3) 0.94183(19) 0.72350(14) 0.0335(6) Uani 1 1 d . . . . .
H23 H 1.012547 0.936289 0.770145 0.040 Uiso 1 1 calc R U . . .
C36 C 0.2961(3) 0.10128(19) 0.61944(13) 0.0301(6) Uani 1 1 d . . . . .
C20 C 0.7934(3) 0.30235(19) 0.60146(14) 0.0326(6) Uani 1 1 d . . . . .
H20 H 0.723686 0.255248 0.605703 0.039 Uiso 1 1 calc R U . . .
C19 C 0.9211(3) 0.27601(19) 0.58128(14) 0.0358(6) Uani 1 1 d . . . . .
H19 H 0.939360 0.210766 0.572510 0.043 Uiso 1 1 calc R U . . .
C2 C 0.7311(3) 0.75867(19) 0.85707(14) 0.0332(6) Uani 1 1 d . . . . .
C6 C 0.8721(3) 0.56364(19) 0.83598(13) 0.0283(5) Uani 1 1 d . . . . .
C30 C 1.2728(3) 0.7546(2) 0.59573(15) 0.0395(7) Uani 1 1 d . . . . .
H30A H 1.221289 0.702997 0.563457 0.059 Uiso 1 1 calc R U . . .
H30B H 1.369647 0.749430 0.587424 0.059 Uiso 1 1 calc R U . . .
H30C H 1.246639 0.815926 0.586999 0.059 Uiso 1 1 calc R U . . .
C29 C 1.3143(3) 0.8319(2) 0.72440(16) 0.0376(6) Uani 1 1 d . . . . .
H29A H 1.282106 0.891448 0.715289 0.056 Uiso 1 1 calc R U . . .
H29B H 1.412126 0.831739 0.717272 0.056 Uiso 1 1 calc R U . . .
H29C H 1.294597 0.826364 0.773466 0.056 Uiso 1 1 calc R U . . .
C26 C 0.9108(3) 0.9601(2) 0.58838(15) 0.0379(7) Uani 1 1 d . . . . .
H26 H 0.885389 0.966436 0.541823 0.045 Uiso 1 1 calc R U . . .
C18 C 1.0222(3) 0.3437(2) 0.57378(15) 0.0367(6) Uani 1 1 d . . . . .
H18 H 1.109627 0.325180 0.559421 0.044 Uiso 1 1 calc R U . . .
C25 C 0.9044(3) 1.0357(2) 0.64440(16) 0.0387(7) Uani 1 1 d . . . . .
H25 H 0.872805 1.093815 0.636546 0.046 Uiso 1 1 calc R U . . .
C9 C 0.9784(3) 0.5102(2) 0.78852(14) 0.0382(7) Uani 1 1 d . . . . .
H9A H 0.941615 0.489685 0.740019 0.057 Uiso 1 1 calc R U . . .
H9B H 1.001221 0.454530 0.807340 0.057 Uiso 1 1 calc R U . . .
H9C H 1.059937 0.552563 0.788011 0.057 Uiso 1 1 calc R U . . .
C5 C 0.6980(3) 0.8337(2) 0.81341(18) 0.0460(8) Uani 1 1 d . . . . .
H5A H 0.781430 0.857853 0.793924 0.069 Uiso 1 1 calc R U . . .
H5B H 0.656332 0.886325 0.844133 0.069 Uiso 1 1 calc R U . . .
H5C H 0.635136 0.804715 0.774385 0.069 Uiso 1 1 calc R U . . .
B1 B 0.4468(3) 0.18835(18) 0.81704(13) 0.0194(5) Uani 1 1 d . . . . .
C8 C 0.9315(3) 0.5932(2) 0.91137(14) 0.0396(7) Uani 1 1 d . . . . .
H8A H 1.007853 0.640352 0.911816 0.059 Uiso 1 1 calc R U . . .
H8B H 0.962878 0.537360 0.927081 0.059 Uiso 1 1 calc R U . . .
H8C H 0.862014 0.620961 0.943536 0.059 Uiso 1 1 calc R U . . .
C31 C 1.2931(3) 0.6545(2) 0.68775(17) 0.0379(7) Uani 1 1 d . . . . .
H31A H 1.279520 0.651597 0.737854 0.057 Uiso 1 1 calc R U . . .
H31B H 1.389527 0.652125 0.677193 0.057 Uiso 1 1 calc R U . . .
H31C H 1.242432 0.600323 0.657633 0.057 Uiso 1 1 calc R U . . .
C3 C 0.8098(4) 0.8110(2) 0.92459(15) 0.0451(7) Uani 1 1 d . . . . .
H3A H 0.840739 0.764493 0.951106 0.068 Uiso 1 1 calc R U . . .
H3B H 0.750570 0.853442 0.954483 0.068 Uiso 1 1 calc R U . . .
H3C H 0.888094 0.848467 0.911053 0.068 Uiso 1 1 calc R U . . .
C24 C 0.9436(3) 1.0276(2) 0.71180(16) 0.0412(7) Uani 1 1 d . . . . .
H24 H 0.941316 1.080393 0.750144 0.049 Uiso 1 1 calc R U . . .
C4 C 0.6014(4) 0.7075(3) 0.8785(2) 0.0548(9) Uani 1 1 d . . . . .
H4A H 0.554435 0.670796 0.835774 0.082 Uiso 1 1 calc R U . . .
H4B H 0.542271 0.754609 0.903437 0.082 Uiso 1 1 calc R U . . .
H4C H 0.624741 0.664633 0.909855 0.082 Uiso 1 1 calc R U . . .
C7 C 0.7449(3) 0.4972(2) 0.8332(2) 0.0544(10) Uani 1 1 d . . . . .
H7A H 0.674213 0.530770 0.861113 0.082 Uiso 1 1 calc R U . . .
H7B H 0.765354 0.441663 0.852904 0.082 Uiso 1 1 calc R U . . .
H7C H 0.713445 0.476317 0.783732 0.082 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -4 12 0.1224
2 -1 -5 0.1125
-3 5 2 0.1176
1 2 -5 0.1460
3 -5 -2 0.1506
2 -3 5 0.1454
-4 -5 -1 0.1065
-3 0 -5 0.1096
-2 3 -5 0.1610
5 5 2 0.1021
3 5 0 0.1207
0 -5 4 0.1648
-5 -3 -4 0.1046
-4 -5 5 0.1118
-5 2 -3 0.1082
5 3 -3 0.1198
4 5 -5 0.1255
5 -3 -1 0.1419
-5 1 4 0.1026
4 1 -5 0.1166
-5 4 0 0.1063
-3 5 -3 0.1486
-2 -2 5 0.1117
-2 2 5 0.1122
0 -1 5 0.1092
0 -1 -5 0.1129
-1 5 5 0.0936
1 1 5 0.0950
-1 -3 -5 0.1143
1 5 5 0.0969
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 S1 Si2 107.86(3) . . ?
C1 P1 S1 114.11(9) . . ?
C1 P1 C2 107.01(11) . . ?
C1 P1 C6 108.74(11) . . ?
C2 P1 S1 105.77(9) . . ?
C2 P1 C6 116.37(12) . . ?
C6 P1 S1 105.06(8) . . ?
O1 Si1 C16 108.87(10) . . ?
O1 Si1 C10 110.25(10) . . ?
O1 Si1 C1 106.42(10) . . ?
C16 Si1 C10 110.60(10) . . ?
C16 Si1 C1 113.90(11) . . ?
C10 Si1 C1 106.69(10) . . ?
O1 Si2 S1 109.26(7) . . ?
O1 Si2 C22 111.27(9) . . ?
O1 Si2 C28 111.02(11) . . ?
C22 Si2 S1 107.97(8) . . ?
C22 Si2 C28 112.77(11) . . ?
C28 Si2 S1 104.22(8) . . ?
Si2 O1 Si1 139.60(11) . . ?
C43 C38 C39 113.2(2) . . ?
C43 C38 B1 127.5(2) . . ?
C39 C38 B1 118.9(2) . . ?
C21 C16 Si1 120.71(18) . . ?
C17 C16 Si1 120.9(2) . . ?
C17 C16 C21 118.4(2) . . ?
C49 C44 C45 112.9(2) . . ?
C49 C44 B1 121.55(18) . . ?
C45 C44 B1 125.2(2) . . ?
F15 C49 C44 119.0(2) . . ?
F15 C49 C48 115.9(2) . . ?
C48 C49 C44 125.1(2) . . ?
F16 C51 C50 119.7(2) . . ?
F16 C51 C52 115.4(2) . . ?
C52 C51 C50 124.9(2) . . ?
F10 C43 C38 121.2(2) . . ?
F10 C43 C42 114.4(2) . . ?
C38 C43 C42 124.4(2) . . ?
C33 C32 C37 112.8(2) . . ?
C33 C32 B1 121.18(18) . . ?
C37 C32 B1 125.8(2) . . ?
F6 C39 C38 120.2(2) . . ?
F6 C39 C40 115.6(2) . . ?
C40 C39 C38 124.3(2) . . ?
C51 C50 B1 119.1(2) . . ?
C55 C50 C51 113.3(2) . . ?
C55 C50 B1 127.0(2) . . ?
C11 C10 Si1 121.22(17) . . ?
C11 C10 C15 118.2(2) . . ?
C15 C10 Si1 120.27(18) . . ?
F11 C45 C44 120.8(2) . . ?
F11 C45 C46 115.56(19) . . ?
C46 C45 C44 123.7(2) . . ?
F14 C48 C49 120.9(2) . . ?
F14 C48 C47 119.8(2) . . ?
C49 C48 C47 119.3(2) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C13 C14 C15 120.2(2) . . ?
F9 C42 C43 120.9(2) . . ?
F9 C42 C41 119.7(2) . . ?
C41 C42 C43 119.3(2) . . ?
F1 C33 C32 119.2(2) . . ?
F1 C33 C34 115.9(2) . . ?
C34 C33 C32 124.9(2) . . ?
F7 C40 C39 119.7(2) . . ?
F7 C40 C41 120.4(2) . . ?
C41 C40 C39 119.9(2) . . ?
C16 C21 H21 119.6 . . ?
C20 C21 C16 120.8(2) . . ?
C20 C21 H21 119.6 . . ?
P1 C1 Si1 124.60(13) . . ?
P1 C1 H1A 106.2 . . ?
P1 C1 H1B 106.2 . . ?
Si1 C1 H1A 106.2 . . ?
Si1 C1 H1B 106.2 . . ?
H1A C1 H1B 106.4 . . ?
F20 C55 C50 121.1(2) . . ?
F20 C55 C54 114.8(2) . . ?
C50 C55 C54 124.0(2) . . ?
F19 C54 C55 120.3(2) . . ?
F19 C54 C53 120.2(2) . . ?
C53 C54 C55 119.5(2) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 C10 120.9(2) . . ?
C12 C11 H11 119.6 . . ?
C27 C22 Si2 120.75(19) . . ?
C27 C22 C23 118.3(2) . . ?
C23 C22 Si2 120.90(17) . . ?
C10 C15 H15 119.6 . . ?
C14 C15 C10 120.8(2) . . ?
C14 C15 H15 119.6 . . ?
F13 C47 C48 120.6(3) . . ?
F13 C47 C46 121.0(2) . . ?
C46 C47 C48 118.4(2) . . ?
F12 C46 C45 119.7(2) . . ?
F12 C46 C47 119.6(2) . . ?
C47 C46 C45 120.6(2) . . ?
F5 C37 C32 120.7(2) . . ?
F5 C37 C36 115.43(19) . . ?
C36 C37 C32 123.9(2) . . ?
C30 C28 Si2 106.78(16) . . ?
C30 C28 C29 110.3(2) . . ?
C30 C28 C31 109.1(2) . . ?
C29 C28 Si2 109.77(19) . . ?
C29 C28 C31 109.2(2) . . ?
C31 C28 Si2 111.65(18) . . ?
C14 C13 H13 120.0 . . ?
C14 C13 C12 120.0(2) . . ?
C12 C13 H13 120.0 . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.8(2) . . ?
C13 C12 H12 120.1 . . ?
C22 C27 H27 119.6 . . ?
C26 C27 C22 120.7(2) . . ?
C26 C27 H27 119.6 . . ?
F17 C52 C51 120.9(3) . . ?
F17 C52 C53 119.9(2) . . ?
C51 C52 C53 119.1(2) . . ?
F18 C53 C54 120.7(3) . . ?
F18 C53 C52 120.1(2) . . ?
C54 C53 C52 119.1(2) . . ?
C16 C17 H17 119.7 . . ?
C16 C17 C18 120.7(3) . . ?
C18 C17 H17 119.7 . . ?
F2 C34 C33 120.9(2) . . ?
F2 C34 C35 119.4(2) . . ?
C33 C34 C35 119.7(2) . . ?
F8 C41 C42 120.7(2) . . ?
F8 C41 C40 120.4(2) . . ?
C40 C41 C42 118.9(2) . . ?
F3 C35 C34 120.9(3) . . ?
F3 C35 C36 120.9(2) . . ?
C36 C35 C34 118.2(2) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 C22 121.0(2) . . ?
C24 C23 H23 119.5 . . ?
F4 C36 C37 120.0(2) . . ?
F4 C36 C35 119.6(2) . . ?
C35 C36 C37 120.4(2) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 C21 119.9(3) . . ?
C19 C20 H20 120.1 . . ?
C20 C19 H19 119.8 . . ?
C18 C19 C20 120.5(2) . . ?
C18 C19 H19 119.8 . . ?
C5 C2 P1 107.35(19) . . ?
C5 C2 C3 107.4(2) . . ?
C3 C2 P1 111.5(2) . . ?
C4 C2 P1 110.0(2) . . ?
C4 C2 C5 111.1(3) . . ?
C4 C2 C3 109.4(3) . . ?
C9 C6 P1 108.23(17) . . ?
C8 C6 P1 109.85(19) . . ?
C8 C6 C9 108.2(2) . . ?
C7 C6 P1 110.55(16) . . ?
C7 C6 C9 108.0(3) . . ?
C7 C6 C8 111.9(3) . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 C27 120.0(2) . . ?
C25 C26 H26 120.0 . . ?
C17 C18 H18 120.1 . . ?
C19 C18 C17 119.8(3) . . ?
C19 C18 H18 120.1 . . ?
C26 C25 H25 119.9 . . ?
C26 C25 C24 120.3(2) . . ?
C24 C25 H25 119.9 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C44 B1 C38 115.06(19) . . ?
C32 B1 C38 112.15(16) . . ?
C32 B1 C44 102.08(18) . . ?
C50 B1 C38 100.34(18) . . ?
C50 B1 C44 113.13(17) . . ?
C50 B1 C32 114.68(19) . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C23 C24 H24 120.1 . . ?
C25 C24 C23 119.8(3) . . ?
C25 C24 H24 120.1 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 P1 2.0678(9) . ?
S1 Si2 2.1940(8) . ?
P1 C1 1.803(2) . ?
P1 C2 1.866(3) . ?
P1 C6 1.868(2) . ?
Si1 O1 1.6381(18) . ?
Si1 C16 1.854(2) . ?
Si1 C10 1.867(2) . ?
Si1 C1 1.899(2) . ?
Si2 O1 1.6265(18) . ?
Si2 C22 1.855(2) . ?
Si2 C28 1.866(3) . ?
F10 C43 1.354(3) . ?
F7 C40 1.357(3) . ?
F6 C39 1.351(3) . ?
F11 C45 1.353(3) . ?
F16 C51 1.354(3) . ?
F20 C55 1.350(3) . ?
F15 C49 1.357(2) . ?
F1 C33 1.358(3) . ?
F5 C37 1.353(3) . ?
F19 C54 1.343(3) . ?
F9 C42 1.340(3) . ?
F8 C41 1.346(3) . ?
F14 C48 1.348(3) . ?
F4 C36 1.356(3) . ?
F12 C46 1.356(3) . ?
F2 C34 1.351(3) . ?
F3 C35 1.346(3) . ?
F18 C53 1.346(3) . ?
F13 C47 1.339(3) . ?
F17 C52 1.336(3) . ?
C38 C43 1.383(3) . ?
C38 C39 1.392(3) . ?
C38 B1 1.659(3) . ?
C16 C21 1.399(4) . ?
C16 C17 1.392(4) . ?
C44 C49 1.387(3) . ?
C44 C45 1.399(3) . ?
C44 B1 1.656(4) . ?
C49 C48 1.377(4) . ?
C51 C50 1.391(3) . ?
C51 C52 1.378(4) . ?
C43 C42 1.394(3) . ?
C32 C33 1.387(3) . ?
C32 C37 1.402(3) . ?
C32 B1 1.655(3) . ?
C39 C40 1.382(3) . ?
C50 C55 1.384(4) . ?
C50 B1 1.654(3) . ?
C10 C11 1.397(3) . ?
C10 C15 1.402(3) . ?
C45 C46 1.378(4) . ?
C48 C47 1.383(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.389(3) . ?
C14 C13 1.385(4) . ?
C42 C41 1.374(4) . ?
C33 C34 1.372(4) . ?
C40 C41 1.369(4) . ?
C21 H21 0.9500 . ?
C21 C20 1.383(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C55 C54 1.395(4) . ?
C54 C53 1.372(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.395(3) . ?
C22 C27 1.391(3) . ?
C22 C23 1.392(4) . ?
C15 H15 0.9500 . ?
C47 C46 1.367(4) . ?
C37 C36 1.375(4) . ?
C28 C30 1.535(4) . ?
C28 C29 1.536(4) . ?
C28 C31 1.537(3) . ?
C13 H13 0.9500 . ?
C13 C12 1.386(4) . ?
C12 H12 0.9500 . ?
C27 H27 0.9500 . ?
C27 C26 1.391(4) . ?
C52 C53 1.381(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.393(4) . ?
C34 C35 1.381(4) . ?
C35 C36 1.371(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.389(4) . ?
C20 H20 0.9500 . ?
C20 C19 1.382(4) . ?
C19 H19 0.9500 . ?
C19 C18 1.378(4) . ?
C2 C5 1.541(4) . ?
C2 C3 1.544(4) . ?
C2 C4 1.536(5) . ?
C6 C9 1.541(4) . ?
C6 C8 1.529(3) . ?
C6 C7 1.524(4) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C26 H26 0.9500 . ?
C26 C25 1.376(4) . ?
C18 H18 0.9500 . ?
C25 H25 0.9500 . ?
C25 C24 1.378(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C24 H24 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 P1 C1 Si1 33.84(18) . . . . ?
S1 P1 C2 C5 71.3(2) . . . . ?
S1 P1 C2 C3 -46.1(2) . . . . ?
S1 P1 C2 C4 -167.7(2) . . . . ?
S1 P1 C6 C9 -53.79(18) . . . . ?
S1 P1 C6 C8 64.1(2) . . . . ?
S1 P1 C6 C7 -171.9(2) . . . . ?
S1 Si2 O1 Si1 39.89(16) . . . . ?
S1 Si2 C22 C27 -156.9(2) . . . . ?
S1 Si2 C22 C23 26.3(2) . . . . ?
S1 Si2 C28 C30 -179.25(17) . . . . ?
S1 Si2 C28 C29 -59.67(17) . . . . ?
S1 Si2 C28 C31 61.6(2) . . . . ?
Si1 C16 C21 C20 -179.71(18) . . . . ?
Si1 C16 C17 C18 179.2(2) . . . . ?
Si1 C10 C11 C12 -171.6(2) . . . . ?
Si1 C10 C15 C14 171.0(2) . . . . ?
Si2 C22 C27 C26 -177.9(2) . . . . ?
Si2 C22 C23 C24 177.5(2) . . . . ?
F10 C43 C42 F9 -1.4(3) . . . . ?
F10 C43 C42 C41 179.1(2) . . . . ?
F7 C40 C41 F8 0.5(4) . . . . ?
F7 C40 C41 C42 -178.1(2) . . . . ?
F6 C39 C40 F7 1.1(3) . . . . ?
F6 C39 C40 C41 -177.7(2) . . . . ?
F11 C45 C46 F12 0.1(3) . . . . ?
F11 C45 C46 C47 179.3(2) . . . . ?
F16 C51 C50 C55 177.56(19) . . . . ?
F16 C51 C50 B1 5.7(3) . . . . ?
F16 C51 C52 F17 2.0(3) . . . . ?
F16 C51 C52 C53 -177.1(2) . . . . ?
F20 C55 C54 F19 1.3(3) . . . . ?
F20 C55 C54 C53 -180.0(2) . . . . ?
F15 C49 C48 F14 -3.0(3) . . . . ?
F15 C49 C48 C47 177.6(2) . . . . ?
F1 C33 C34 F2 -1.8(4) . . . . ?
F1 C33 C34 C35 177.0(2) . . . . ?
F5 C37 C36 F4 -0.6(4) . . . . ?
F5 C37 C36 C35 178.9(2) . . . . ?
F19 C54 C53 F18 0.2(4) . . . . ?
F19 C54 C53 C52 178.0(2) . . . . ?
F9 C42 C41 F8 0.2(4) . . . . ?
F9 C42 C41 C40 178.8(2) . . . . ?
F14 C48 C47 F13 1.2(4) . . . . ?
F14 C48 C47 C46 179.7(2) . . . . ?
F2 C34 C35 F3 0.2(4) . . . . ?
F2 C34 C35 C36 178.7(2) . . . . ?
O1 Si1 C16 C21 167.79(17) . . . . ?
O1 Si1 C16 C17 -11.9(2) . . . . ?
O1 Si1 C10 C11 115.3(2) . . . . ?
O1 Si1 C10 C15 -58.5(2) . . . . ?
O1 Si1 C1 P1 -34.68(17) . . . . ?
O1 Si2 C22 C27 -37.0(3) . . . . ?
O1 Si2 C22 C23 146.2(2) . . . . ?
O1 Si2 C28 C30 63.2(2) . . . . ?
O1 Si2 C28 C29 -177.18(16) . . . . ?
O1 Si2 C28 C31 -56.0(2) . . . . ?
F3 C35 C36 F4 -0.6(4) . . . . ?
F3 C35 C36 C37 179.9(2) . . . . ?
F13 C47 C46 F12 0.2(4) . . . . ?
F13 C47 C46 C45 -179.1(2) . . . . ?
F17 C52 C53 F18 -2.0(4) . . . . ?
F17 C52 C53 C54 -179.8(2) . . . . ?
C38 C43 C42 F9 -179.6(2) . . . . ?
C38 C43 C42 C41 0.8(4) . . . . ?
C38 C39 C40 F7 -179.9(2) . . . . ?
C38 C39 C40 C41 1.3(4) . . . . ?
C16 Si1 O1 Si2 -132.20(15) . . . . ?
C16 Si1 C10 C11 -5.1(2) . . . . ?
C16 Si1 C10 C15 -179.0(2) . . . . ?
C16 Si1 C1 P1 85.27(18) . . . . ?
C16 C21 C20 C19 0.8(4) . . . . ?
C16 C17 C18 C19 0.2(4) . . . . ?
C44 C49 C48 F14 178.0(2) . . . . ?
C44 C49 C48 C47 -1.4(4) . . . . ?
C44 C45 C46 F12 179.0(2) . . . . ?
C44 C45 C46 C47 -1.8(4) . . . . ?
C49 C44 C45 F11 178.4(2) . . . . ?
C49 C44 C45 C46 -0.4(3) . . . . ?
C49 C44 B1 C38 47.3(3) . . . . ?
C49 C44 B1 C32 -74.4(3) . . . . ?
C49 C44 B1 C50 161.8(2) . . . . ?
C49 C48 C47 F13 -179.4(2) . . . . ?
C49 C48 C47 C46 -0.9(4) . . . . ?
C51 C50 C55 F20 -178.81(19) . . . . ?
C51 C50 C55 C54 -0.2(3) . . . . ?
C51 C50 B1 C38 72.7(2) . . . . ?
C51 C50 B1 C44 -50.4(3) . . . . ?
C51 C50 B1 C32 -166.89(19) . . . . ?
C51 C52 C53 F18 177.0(2) . . . . ?
C51 C52 C53 C54 -0.8(4) . . . . ?
C43 C38 C39 F6 176.93(19) . . . . ?
C43 C38 C39 C40 -2.0(3) . . . . ?
C43 C38 B1 C44 21.9(3) . . . . ?
C43 C38 B1 C32 137.9(2) . . . . ?
C43 C38 B1 C50 -99.9(3) . . . . ?
C43 C42 C41 F8 179.7(2) . . . . ?
C43 C42 C41 C40 -1.6(4) . . . . ?
C32 C33 C34 F2 178.8(2) . . . . ?
C32 C33 C34 C35 -2.4(4) . . . . ?
C32 C37 C36 F4 -179.9(2) . . . . ?
C32 C37 C36 C35 -0.4(4) . . . . ?
C39 C38 C43 F10 -177.19(19) . . . . ?
C39 C38 C43 C42 0.9(3) . . . . ?
C39 C38 B1 C44 -165.67(19) . . . . ?
C39 C38 B1 C32 -49.6(3) . . . . ?
C39 C38 B1 C50 72.6(2) . . . . ?
C39 C40 C41 F8 179.3(2) . . . . ?
C39 C40 C41 C42 0.7(4) . . . . ?
C50 C51 C52 F17 -178.9(2) . . . . ?
C50 C51 C52 C53 2.1(4) . . . . ?
C50 C55 C54 F19 -177.5(2) . . . . ?
C50 C55 C54 C53 1.3(4) . . . . ?
C10 Si1 O1 Si2 106.30(16) . . . . ?
C10 Si1 C16 C21 -70.9(2) . . . . ?
C10 Si1 C16 C17 109.4(2) . . . . ?
C10 Si1 C1 P1 -152.40(15) . . . . ?
C10 C11 C12 C13 0.1(4) . . . . ?
C45 C44 C49 F15 -176.9(2) . . . . ?
C45 C44 C49 C48 2.0(3) . . . . ?
C45 C44 B1 C38 -140.3(2) . . . . ?
C45 C44 B1 C32 98.0(2) . . . . ?
C45 C44 B1 C50 -25.8(3) . . . . ?
C48 C47 C46 F12 -178.3(2) . . . . ?
C48 C47 C46 C45 2.4(4) . . . . ?
C14 C13 C12 C11 -2.1(4) . . . . ?
C33 C32 C37 F5 178.9(2) . . . . ?
C33 C32 C37 C36 -1.9(4) . . . . ?
C33 C32 B1 C38 161.0(2) . . . . ?
C33 C32 B1 C44 -75.3(3) . . . . ?
C33 C32 B1 C50 47.4(3) . . . . ?
C33 C34 C35 F3 -178.6(2) . . . . ?
C33 C34 C35 C36 -0.1(4) . . . . ?
C21 C16 C17 C18 -0.5(4) . . . . ?
C21 C20 C19 C18 -1.1(4) . . . . ?
C1 P1 C2 C5 -50.7(2) . . . . ?
C1 P1 C2 C3 -168.1(2) . . . . ?
C1 P1 C2 C4 70.3(2) . . . . ?
C1 P1 C6 C9 68.8(2) . . . . ?
C1 P1 C6 C8 -173.33(19) . . . . ?
C1 P1 C6 C7 -49.4(3) . . . . ?
C1 Si1 O1 Si2 -9.04(17) . . . . ?
C1 Si1 C16 C21 49.2(2) . . . . ?
C1 Si1 C16 C17 -130.43(19) . . . . ?
C1 Si1 C10 C11 -129.5(2) . . . . ?
C1 Si1 C10 C15 56.7(2) . . . . ?
C55 C50 B1 C38 -97.9(2) . . . . ?
C55 C50 B1 C44 139.0(2) . . . . ?
C55 C50 B1 C32 22.4(3) . . . . ?
C55 C54 C53 F18 -178.6(2) . . . . ?
C55 C54 C53 C52 -0.8(4) . . . . ?
C11 C10 C15 C14 -3.0(4) . . . . ?
C22 Si2 O1 Si1 -79.24(17) . . . . ?
C22 Si2 C28 C30 -62.4(2) . . . . ?
C22 Si2 C28 C29 57.2(2) . . . . ?
C22 Si2 C28 C31 178.40(18) . . . . ?
C22 C27 C26 C25 0.1(5) . . . . ?
C22 C23 C24 C25 0.6(5) . . . . ?
C15 C10 C11 C12 2.4(4) . . . . ?
C15 C14 C13 C12 1.5(4) . . . . ?
C37 C32 C33 F1 -176.1(2) . . . . ?
C37 C32 C33 C34 3.2(4) . . . . ?
C37 C32 B1 C38 -25.0(3) . . . . ?
C37 C32 B1 C44 98.7(3) . . . . ?
C37 C32 B1 C50 -138.6(2) . . . . ?
C28 Si2 O1 Si1 154.29(14) . . . . ?
C28 Si2 C22 C27 88.5(2) . . . . ?
C28 Si2 C22 C23 -88.3(2) . . . . ?
C13 C14 C15 C10 1.1(4) . . . . ?
C27 C22 C23 C24 0.7(4) . . . . ?
C27 C26 C25 C24 1.3(5) . . . . ?
C52 C51 C50 C55 -1.6(3) . . . . ?
C52 C51 C50 B1 -173.5(2) . . . . ?
C17 C16 C21 C20 0.0(3) . . . . ?
C34 C35 C36 F4 -179.1(2) . . . . ?
C34 C35 C36 C37 1.4(4) . . . . ?
C23 C22 C27 C26 -1.1(4) . . . . ?
C20 C19 C18 C17 0.6(4) . . . . ?
C2 P1 C1 Si1 150.47(15) . . . . ?
C2 P1 C6 C9 -170.37(18) . . . . ?
C2 P1 C6 C8 -52.5(2) . . . . ?
C2 P1 C6 C7 71.5(3) . . . . ?
C6 P1 C1 Si1 -83.06(18) . . . . ?
C6 P1 C2 C5 -172.47(19) . . . . ?
C6 P1 C2 C3 70.1(2) . . . . ?
C6 P1 C2 C4 -51.5(3) . . . . ?
C26 C25 C24 C23 -1.6(5) . . . . ?
B1 C38 C43 F10 -4.4(3) . . . . ?
B1 C38 C43 C42 173.8(2) . . . . ?
B1 C38 C39 F6 3.4(3) . . . . ?
B1 C38 C39 C40 -175.5(2) . . . . ?
B1 C44 C49 F15 -3.7(3) . . . . ?
B1 C44 C49 C48 175.3(2) . . . . ?
B1 C44 C45 F11 5.4(3) . . . . ?
B1 C44 C45 C46 -173.4(2) . . . . ?
B1 C32 C33 F1 -1.4(4) . . . . ?
B1 C32 C33 C34 178.0(2) . . . . ?
B1 C32 C37 F5 4.5(4) . . . . ?
B1 C32 C37 C36 -176.3(2) . . . . ?
B1 C50 C55 F20 -7.7(3) . . . . ?
B1 C50 C55 C54 171.0(2) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.2826 -4.1293 11.7211 -0.5873 0.1085 0.8020
2.0072 -0.9951 -5.0036 0.5215 -0.0623 -0.0979
-2.9980 4.9939 2.0001 -0.6346 0.0780 -0.3633
1.0104 2.0024 -5.0041 0.2898 0.0211 -0.3511
2.9980 -4.9939 -2.0001 0.6346 -0.0780 0.3633
1.9889 -3.0005 5.0064 0.0704 0.2500 0.4922
-4.0045 -4.9971 -1.0046 -0.1616 -0.8184 0.2582
-2.9924 0.0024 -5.0074 -0.0509 -0.5576 -0.2814
-1.9889 3.0005 -5.0064 -0.0704 -0.2500 -0.4922
5.0031 4.9968 2.0064 0.2142 0.9747 -0.1934
3.0060 4.9975 0.0028 0.1090 0.6620 -0.3230
-0.0120 -4.9991 4.0036 -0.0046 -0.1487 0.5608
-4.9976 -2.9969 -4.0082 -0.1910 -0.9329 -0.0484
-4.0142 -5.0013 5.0015 -0.4825 -0.5528 0.5194
-4.9936 1.9988 -3.0068 -0.4538 -0.5629 -0.3915
5.0089 3.0017 -2.9989 0.5654 0.6231 -0.2564
4.0142 5.0013 -5.0015 0.4825 0.5528 -0.5194
4.9990 -2.9953 -0.9974 0.7096 0.3207 0.2947
-5.0060 0.9946 4.0003 -0.7863 -0.3182 -0.0094
4.0097 1.0042 -5.0019 0.6500 0.2922 -0.2101
-4.9962 3.9952 -0.0036 -0.6980 -0.2998 -0.4156
-2.9900 4.9973 -3.0050 -0.3672 -0.1433 -0.5810
-2.0106 -2.0027 5.0034 -0.3959 -0.1332 0.3299
-2.0061 1.9943 5.0037 -0.5634 0.1274 0.0205
-0.0092 -1.0027 5.0050 -0.2256 0.1562 0.2950
0.0069 -0.9958 -5.0052 0.3093 -0.2865 -0.1404
-1.0026 4.9925 5.0048 -0.5828 0.4350 -0.1902
0.9932 0.9962 5.0060 -0.2032 0.3985 0.1616
-0.9954 -2.9947 -5.0061 0.2869 -0.5288 -0.0069
0.9977 4.9933 5.0063 -0.3706 0.6591 -0.1477
